JP2000155081A - Sample generating device and method - Google Patents
Sample generating device and methodInfo
- Publication number
- JP2000155081A JP2000155081A JP10332237A JP33223798A JP2000155081A JP 2000155081 A JP2000155081 A JP 2000155081A JP 10332237 A JP10332237 A JP 10332237A JP 33223798 A JP33223798 A JP 33223798A JP 2000155081 A JP2000155081 A JP 2000155081A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- probe
- sample piece
- holder
- observation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000523 sample Substances 0.000 claims abstract description 385
- 238000012545 processing Methods 0.000 claims abstract description 29
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 26
- 230000003287 optical effect Effects 0.000 claims abstract description 5
- 230000005540 biological transmission Effects 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 28
- 238000005464 sample preparation method Methods 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 13
- 238000012546 transfer Methods 0.000 claims description 10
- 230000001678 irradiating effect Effects 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 6
- 230000005489 elastic deformation Effects 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000009434 installation Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 230000005855 radiation Effects 0.000 abstract 1
- 239000008188 pellet Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- 230000000007 visual effect Effects 0.000 description 7
- 239000010408 film Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 125000006850 spacer group Chemical group 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、微細構造が形成さ
れた半導体ウエハ、磁気ヘッド等の表面から、透過型電
子顕微鏡（Transmission Electron Microscope：以下TE
Mと略記）、走査型電子顕微鏡（Scanning Electron Mic
roscope：以下SEMと略記）による観察に必要な微細寸法
の試料片を、集束イオンビーム（Focused Ion Beam：以
下FIBと略記）を用いて加工、採取する試料作成方法お
よび試料作成装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a transmission electron microscope (hereinafter referred to as TE) from a surface of a semiconductor wafer, a magnetic head or the like on which a fine structure is formed.
M), Scanning Electron Mic
The present invention relates to a sample preparation method and a sample preparation apparatus for processing and collecting a sample piece having a fine dimension required for observation by a roscope (hereinafter abbreviated as SEM) using a focused ion beam (hereinafter abbreviated as FIB).
【０００２】[0002]
【従来の技術】FIBを用いたTEMの観察試料の作成方法に
は、例えば、E.C.G.Kirkらが、論文集Microscopy of Se
miconducting Materials 1989， Institute of Physics
No.100， p.501−506 において説明されているような
方法がある。2. Description of the Related Art For example, ECG Kirk et al.
miconducting Materials 1989, Institute of Physics
No. 100, p.501-506.
【０００３】図９でこの従来の技術を説明する。観察対
象となるウエハ101から短冊状ペレット102（試料）をダ
イシングによって、およそ3×0.1×0.5mm（ウエハの厚
み）に切り出す（ペレット切り出し工程）。次に半円形
金属板103の端面に短冊状ペレット102を固定する（ペレ
ット固定工程）。この状態でFIBによって厚さ100nm程度
の薄膜状に加工する（ペレット成形工程）。これを図示
したのが短冊状ペレット102′である。そして、TEM観察
用ホルダ104に半円形金属板103を人手によって設置して
（試料設置工程）TEM観察を行なう。FIG. 9 illustrates this conventional technique. A strip-shaped pellet 102 (sample) is cut out from the wafer 101 to be observed by dicing to a size of about 3 × 0.1 × 0.5 mm (wafer thickness) (pellet cutting step). Next, the strip-shaped pellet 102 is fixed to the end surface of the semicircular metal plate 103 (pellet fixing step). In this state, it is processed into a thin film having a thickness of about 100 nm by FIB (pellet forming step). This is shown as a strip-shaped pellet 102 '. Then, the semicircular metal plate 103 is manually set on the TEM observation holder 104 (sample setting step) to perform TEM observation.
【０００４】[0004]
【発明が解決しようとする課題】まず上記の従来技術に
おいて、ペレット切り出し工程から始まって試料設置工
程を完了するまでに3〜5時間という長時間の処理を行な
わなければならないということがある。また、ペレット
や半円形金属板は非常に小さく、人手で扱うには熟練が
要求され、試料作成のためのコストが高くなる要因とな
っている。First, in the above-mentioned prior art, there is a case where a long process of 3 to 5 hours must be performed from the pellet cutting step to the completion of the sample setting step. In addition, pellets and semicircular metal plates are very small and require skill for manual handling, which is a factor that increases the cost for sample preparation.
【０００５】本発明ではこの問題を解決するため、一連
の試料作成工程を簡略化するとともに、作成作業の殆ど
を自動化可能な試料作成装置および方法を提供すること
によって、時間短縮およびコストの低減を行なうことを
目的としている。In order to solve this problem, the present invention simplifies a series of sample preparation steps and provides a sample preparation apparatus and method capable of automating most of the preparation operations, thereby reducing time and cost. It is intended to do.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成するため
に、本発明においては次のような手段を講じる。本発明
による試料作成装置は、試料処理室にFIBと、二次電子
検出器と、デポジション用ガス源と、試料移動機構と、
試料片を採取するための試料片プローブと、試料片プロ
ーブを着脱可能な試料片プローブホルダおよび試料片プ
ローブ移動機構と、試料片プローブ単体を搭載する観察
用試料ホルダおよび観察用試料ホルダ移動機構を設置す
ることで構成される。To achieve the above object, the present invention takes the following measures. The sample preparation device according to the present invention, the FIB in the sample processing chamber, a secondary electron detector, a gas source for deposition, a sample moving mechanism,
A sample piece probe for collecting a sample piece, a sample piece probe holder and a sample piece probe moving mechanism to which the sample piece probe can be attached and detached, and an observation sample holder and an observation sample holder moving mechanism for mounting the sample piece probe alone. It is composed by installing.
【０００７】次に、上記の試料作成装置の構成要素によ
る試料作成方法を説明する。本発明による試料作成の一
連の工程は、元試料にレーザ等で加工目標位置をマーキ
ングを行なうマーキング工程、試料処理室内においてあ
らかじめ観察用試料ホルダに設置されている試料片プロ
ーブをFIBによる視野観察によって、試料片プローブホ
ルダに持ち替える試料片プローブ持ち替え工程、所望の
形状に元試料から試料片を成形する試料片成形工程、成
形後の試料片に試料片プローブ先端を接触させるための
試料片プローブ接触工程、集束イオンビームとデポジシ
ョン用ガスの照射による試料片と試料片プローブ先端の
試料片接続工程、集束イオンビームの照射によって試料
片と元試料を分離する試料片分離工程、試料片プローブ
を観察用試料ホルダ10に移載する試料片プローブ移載工
程によって行われる。Next, a description will be given of a sample preparation method using the components of the above-described sample preparation apparatus. A series of steps for preparing a sample according to the present invention includes a marking step of marking a processing target position on an original sample with a laser or the like, and a sample piece probe previously set in an observation sample holder in a sample processing chamber by visual field observation using a FIB. A sample piece probe holding step of changing to a sample piece probe holder, a sample piece forming step of forming a sample piece from an original sample into a desired shape, a sample piece probe contacting step of bringing the tip of the sample piece probe into contact with the formed sample piece , A sample piece connecting step between the sample piece and the tip of the sample piece probe by irradiating the focused ion beam and the deposition gas, a sample piece separating step of separating the sample piece from the original sample by irradiating the focused ion beam, and observing the sample piece probe This is performed in a sample piece probe transfer step of transferring the sample piece to the sample holder 10.
【０００８】また、以上説明したような試料作成方法に
おいて、TEM観察のための試料を作成する場合は、上記
工程に加えて、試料片分離工程と試料片プローブ移載工
程の間に試料片の中央部に集束イオンビームを照射する
ことによって、100nm程度の厚みの薄壁部を形成する薄
壁部形成工程を付加する。In the above-described sample preparation method, when preparing a sample for TEM observation, in addition to the above-described steps, the sample piece is separated between the sample piece separation step and the sample piece probe transfer step. A thin-wall portion forming step of forming a thin-wall portion having a thickness of about 100 nm by irradiating the focused ion beam to the central portion is added.
【０００９】[0009]
【発明の実施の形態】図１および図２は本発明による試
料作成装置の基本構成を示す概略図である。図１におい
て真空排気機能を有する試料処理室1には、試料片の加
工および加工部近傍の画像観察を行なうための集束イオ
ンビーム（FIB）照射光学系2および二次電子検出器3
と、集束イオンビームの照射領域にデポジション膜を形
成するためのデポジション用ガス源4と、元試料5が設置
され、イオンビームに対する相対変位を与えるための試
料移動機構6と、試料片を採取するための試料片プロー
ブ7と、試料片プローブ7を着脱可能な試料片プローブホ
ルダ8および試料片プローブ移動機構9と、試料片プロー
ブ7単体を搭載する観察用試料ホルダ10および観察用試
料ホルダ移動機構11が設置されている。1 and 2 are schematic views showing the basic configuration of a sample preparation apparatus according to the present invention. In FIG. 1, a sample processing chamber 1 having an evacuation function is provided with a focused ion beam (FIB) irradiation optical system 2 and a secondary electron detector 3 for processing a sample piece and observing an image near a processed portion.
And a deposition gas source 4 for forming a deposition film in the irradiation area of the focused ion beam, a sample moving mechanism 6 for providing a relative displacement with respect to the ion beam in which an original sample 5 is provided, and a sample piece. A sample probe 7 for sampling, a sample probe holder 8 and a sample probe moving mechanism 9 to which the sample probe 7 can be attached and detached, and an observation sample holder 10 and an observation sample holder on which the sample probe 7 alone is mounted. A moving mechanism 11 is provided.
【００１０】また、図２において、試料片プローブ7
は、試料片プローブホルダ8との結合部となるチャック
プレート12と、傾斜スペーサ13と、試料片15を保持する
カンチレバー14が一体として結合されることによって構
成される。ここで、カンチレバー14は傾斜スペーサ13に
よってチャックプレート12と15〜20°の逃げ角を持って
いることが必要である。これは、TEMの電子線が図面上
で垂直に照射される場合、試料片プローブ7も垂直に設
置されなければならず、適当な逃げ角がないとカンチレ
バー14によって透過電子線の散乱が妨げられるためであ
る。In FIG. 2, the sample piece probe 7
Is configured by integrally connecting a chuck plate 12 serving as a connection portion with the sample piece probe holder 8, an inclined spacer 13, and a cantilever 14 holding a sample piece 15. Here, it is necessary that the cantilever 14 has a clearance angle of 15 to 20 ° with the chuck plate 12 by the inclined spacer 13. This is because when the TEM electron beam is irradiated vertically on the drawing, the sample probe 7 must also be installed vertically, and scattering of the transmitted electron beam is prevented by the cantilever 14 without an appropriate clearance angle. That's why.
【００１１】次に、上記の試料作成装置の構成要素によ
る第１の試料作成方法について説明する。図３、図４お
よび図５は本発明による第１試料作成方法の概略を示し
た図である。Next, a first sample preparation method using the components of the sample preparation apparatus will be described. FIGS. 3, 4 and 5 are diagrams schematically showing a first sample preparation method according to the present invention.
【００１２】図３（a）は集束イオンビームによって試
料片15を成形加工する方法を示したものである。まず、
あらかじめ元試料5にレーザ等で加工目標位置のマーキ
ングを行なう（マーキング工程、図示せず）。一方、図
５で示すように、試料処理室1内においてあらかじめ観
察用試料ホルダ10に設置されている試料片プローブ7を
集束イオンビームによる視野観察によって、試料片プロ
ーブホルダ8に持ち替える（試料片プローブ持ち替え工
程）。ここでの、試料片プローブホルダ8および観察用
試料ホルダ10の位置合わせのための移動は、図１の試料
片プローブ移動機構9および観察用試料ホルダ移動機構1
1によって行なう。FIG. 3A shows a method of forming a sample 15 by a focused ion beam. First,
The target target position is previously marked on the original sample 5 with a laser or the like (marking process, not shown). On the other hand, as shown in FIG. 5, the sample probe 7 previously set in the observation sample holder 10 in the sample processing chamber 1 is replaced by the sample probe holder 8 by visual field observation using a focused ion beam (sample probe). Switching process). Here, the movement for positioning the sample piece probe holder 8 and the observation sample holder 10 is performed by the sample piece probe moving mechanism 9 and the observation sample holder moving mechanism 1 shown in FIG.
Perform by 1.
【００１３】元試料5を試料処理室1に搬送し、試料移動
機構6によってマーキング位置とビーム位置を合わせ
る。次に集束イオンビームの照射によって、図３（a）
の円内を拡大して示す加工部平面図に示すような矩形の
垂直加工部および傾斜加工部の組み合わせにより、ハッ
チングを施した領域で元試料5の除去加工を行なう。こ
の傾斜加工の場合は試料移動機構6を傾斜させて行な
う。これによって、片持ち状態の部分でつながった試料
片15を形成することができる（試料片成形工程）。The original sample 5 is transported to the sample processing chamber 1, and the marking position and the beam position are adjusted by the sample moving mechanism 6. Next, by irradiation of the focused ion beam, FIG.
The original sample 5 is removed in the hatched area by a combination of a rectangular vertical processing part and an inclined processing part as shown in the processing part plan view in which the inside of the circle is enlarged. In the case of the tilt processing, the sample moving mechanism 6 is tilted. Thus, the connected sample pieces 15 can be formed in the cantilevered state (sample piece forming step).
【００１４】図３（b）は成形後の試料片15に試料片プ
ローブ7を接近させ、カンチレバー14の先端を接触させ
た状態を示すものである。ここでの接近方法は、あくま
で視野の中心に試料片15を固定し、試料片プローブ移動
機構9の三次元的な精密移動によって接近および接触を
行なう。カンチレバー14の先端形状は試料片15の両端と
垂直加工部を渡って元試料5の表面に接触させることが
できる形状にする。これは、カンチレバー14の接触端が
元試料5に接触したとき、元試料5の表面に支持され、片
持ち状態の試料片15を押さえすぎて上記片持ち状部分を
破損しないようにするためである（試料片プローブ接触
工程）。FIG. 3B shows a state in which the sample probe 7 is brought close to the molded sample 15 and the tip of the cantilever 14 is brought into contact. In this approach, the sample piece 15 is fixed at the center of the field of view, and approach and contact are performed by three-dimensional precision movement of the sample piece probe moving mechanism 9. The tip of the cantilever 14 is shaped so that it can contact the surface of the original sample 5 across both ends of the sample piece 15 and the vertical processing portion. This is because when the contact end of the cantilever 14 comes into contact with the original sample 5, the cantilever 14 is supported on the surface of the original sample 5 so that the cantilever 14 is not pressed too much and the cantilever portion is damaged. Yes (sample probe contact step).
【００１５】図４（a）ではカンチレバー14の接触端と
試料片15を接続し、試料片15を元試料5から分離する方
法をに示す。集束イオンビームの照射領域をカンチレバ
ー14の接触端と試料片15に渡る領域（黒丸指示部）に設
定する。そして、上記照射領域にデポジション用ガス源
4から、例えばヘキサカルボニルタングステン（W（CO）
6）などのデポジション用ガスを照射し、上記接触端と
試料片15上にタングステン膜を形成することによって両
者を接続する（試料片接続工程）。FIG. 4A shows a method of connecting the contact end of the cantilever 14 and the sample piece 15 and separating the sample piece 15 from the original sample 5. The irradiation area of the focused ion beam is set to an area (a black circle indicating portion) extending between the contact end of the cantilever 14 and the sample piece 15. Then, a deposition gas source is provided in the irradiation area.
From 4, for example, hexacarbonyl tungsten (W (CO)
A deposition gas such as 6 ) is irradiated, and a tungsten film is formed on the contact end and the sample piece 15 to connect them (sample piece connecting step).
【００１６】次に、集束イオンビームの照射によって前
記片持ち状態部分の除去加工を行ない、試料片15を元試
料5から分離する（試料片分離工程）。Next, the cantilevered portion is removed by irradiation with a focused ion beam to separate the sample piece 15 from the original sample 5 (sample piece separation step).
【００１７】次に、図５で示すように、試料片プローブ
ホルダ8で保持されている試料片プローブ7を集束イオン
ビームによる視野観察によって観察用試料ホルダ10に移
載する（試料片プローブ移載工程）。Next, as shown in FIG. 5, the sample probe 7 held by the sample probe holder 8 is transferred to the observation sample holder 10 by visual field observation using a focused ion beam (sample probe transfer). Process).
【００１８】以上説明したような試料作成方法におい
て、TEM観察のための試料を作成する場合は、上記工程
に加えて、試料片分離工程と試料片プローブ移載工程の
間に図４（b）に示すように、試料片15の中央部に集束
イオンビームを照射することによって、100nm程度の厚
みの薄壁部を形成する（薄壁部形成工程）。In the sample preparation method described above, when preparing a sample for TEM observation, in addition to the above-described steps, a sample piece separation step and a sample piece probe transfer step are performed as shown in FIG. As shown in (1), a thin wall portion having a thickness of about 100 nm is formed by irradiating a focused ion beam to the center of the sample piece 15 (thin wall portion forming step).
【００１９】以上説明した試料作成装置および試料作成
方法は、ウエハ（6〜12inサイズ）等のように比較的大
きな元試料を試料移動機構に設置して試料片を作成する
場合に好適であるが、チップ（5mm角程度）等の比較的
小さい元試料を取り扱う場合は、以下に説明する試料作
成装置を用いた試料作成方法を行なうことが効果的であ
る。The sample preparation apparatus and the sample preparation method described above are suitable for the case where a relatively large original sample such as a wafer (6 to 12 inches in size) or the like is installed in a sample moving mechanism to prepare a sample piece. When handling a relatively small original sample such as a chip (about 5 mm square) or the like, it is effective to perform a sample preparation method using a sample preparation apparatus described below.
【００２０】図６は本発明による第２の試料作成装置の
基本構成を示す概略図である。図６において真空排気機
能を有する試料処理室1には、試料片の加工および加工
部近傍の画像観察を行なうための集束イオンビーム（FI
B）照射光学系2および二次電子検出器3と、集束イオン
ビームの照射領域にデポジション膜を形成するためのデ
ポジション用ガス源4と、試料片15を採取するための試
料片プローブ7と、試料片プローブ7を着脱可能な試料片
プローブホルダ8および試料片プローブ移動機構9と、試
料片プローブ7単体と元試料17を搭載する観察用試料ホ
ルダ16および観察用試料ホルダ移動機構18が設置されて
いる。FIG. 6 is a schematic diagram showing the basic configuration of a second sample preparation apparatus according to the present invention. In FIG. 6, a sample processing chamber 1 having a vacuum evacuation function is provided with a focused ion beam (FI
B) Irradiation optical system 2 and secondary electron detector 3, deposition gas source 4 for forming a deposition film in the irradiation region of the focused ion beam, and sample probe 7 for collecting sample 15 A sample piece probe holder 8 and a sample piece probe moving mechanism 9 to which the sample piece probe 7 can be attached and detached, and an observation sample holder 16 and an observation sample holder moving mechanism 18 for mounting the sample piece probe 7 alone and the original sample 17 are provided. is set up.
【００２１】次に、上記の第２の試料作成装置の構成要
素による第２の試料作成方法を第１の試料作成方法と比
較しながら図７で説明する。あらかじめ元試料17にレー
ザ等で加工目標位置のマーキングを行ない（マーキング
工程）、元試料17を試料片プローブ7とともに観察用試
料ホルダ16に設置した後、試料処理室1に導入する。Next, a second sample preparation method using the components of the second sample preparation apparatus will be described with reference to FIG. 7 in comparison with the first sample preparation method. The target target position is marked on the original sample 17 in advance with a laser or the like (marking step). The original sample 17 is placed on the observation sample holder 16 together with the sample piece probe 7 and then introduced into the sample processing chamber 1.
【００２２】次に、図７（a）で示すように、観察用試
料ホルダ16に設置されている試料片プローブ7を集束イ
オンビームによる視野観察によって、試料片プローブホ
ルダ8に持ち替える（試料片プローブ持ち替え工程）。
ここでの、試料片プローブホルダ8および観察用試料ホ
ルダ16の位置合わせのための移動は、図６の試料片プロ
ーブ移動機構9および観察用試料ホルダ移動機構18によ
って行なう。Next, as shown in FIG. 7A, the sample piece probe 7 installed in the observation sample holder 16 is changed to the sample piece probe holder 8 by visual field observation using a focused ion beam (sample piece probe). Switching process).
The movement for positioning the sample piece probe holder 8 and the observation sample holder 16 here is performed by the sample piece probe moving mechanism 9 and the observation sample holder moving mechanism 18 in FIG.
【００２３】次に、観察用試料ホルダ移動機構18によっ
て観察用試料ホルダ16に設置されている元試料17のマー
キング位置とビーム位置を合わせる。以下、試料片成形
工程、試料片プローブ接触工程、試料片接続工程、試料
片分離工程は、図７（b）に示すように、観察用試料ホ
ルダ16上で行われること以外は前記第１の試料作成方法
と同じである。Next, the marking position of the original sample 17 placed on the observation sample holder 16 and the beam position are adjusted by the observation sample holder moving mechanism 18. Hereinafter, except that the sample piece forming step, the sample piece probe contacting step, the sample piece connecting step, and the sample piece separating step are performed on the observation sample holder 16 as shown in FIG. It is the same as the sample preparation method.
【００２４】次に、図７（c）に示すように、試料片プ
ローブホルダ8で保持されている試料片プローブ7を集束
イオンビームによる視野観察によって観察用試料ホルダ
16に移載する（試料片プローブ移載工程）。Next, as shown in FIG. 7C, the specimen probe 7 held by the specimen probe holder 8 is observed by a visual field observation using a focused ion beam.
Transfer to 16 (sample probe transfer process).
【００２５】以上説明したような第２の試料作成方法に
おいても、TEM観察のための試料を作成する場合は、上
記工程に加えて、試料片分離工程と試料片プローブ移載
工程の間に図４（b）に示すように、試料片15の中央部
に集束イオンビームを照射することによって、100nm程
度の厚みの薄壁部を形成する（薄壁部形成工程）。In the second sample preparation method as described above, when preparing a sample for TEM observation, in addition to the above-described steps, it is also necessary to set the time between the sample piece separation step and the sample piece probe transfer step. As shown in FIG. 4B, a thin wall portion having a thickness of about 100 nm is formed by irradiating a focused ion beam to a central portion of the sample piece 15 (thin wall portion forming step).
【００２６】ところで、上記第１の試料作成方法および
第２の試料作成方法における試料片プローブ接触工程で
は、視野観察によって試料片プローブ7の先端を平面的
に位置合わせすることは比較的正確に行なえるが、垂直
方向の位置情報が得にくいため、正確に接触させること
が困難である。By the way, in the sample probe contacting step in the first sample preparation method and the second sample preparation method, it is relatively accurate to position the tip of the sample probe 7 in a planar manner by visual field observation. However, since it is difficult to obtain vertical position information, it is difficult to make accurate contact.
【００２７】そのため視野観察に加えて、試料片プロー
ブ7の先端が元試料5または17の表面に接触したことを検
知する手段を備えることが望ましい。Therefore, it is desirable to provide a means for detecting that the tip of the sample piece probe 7 has come into contact with the surface of the original sample 5 or 17 in addition to the visual field observation.
【００２８】図８は試料片プローブの先端の接触検知の
手段の一例を示した図である。第１の手段は図８（a）
に示すように、試料片プローブホルダ8の裏面に圧電素
子23を設置し、試料片プローブホルダ8の共振状態の超
音波振動を圧電素子23によって与え、試料片プローブ7
の先端の接触による共振状態の乱れを測定することによ
って接触検知を行なうことができる。FIG. 8 is a diagram showing an example of the means for detecting the contact of the tip of the sample piece probe. The first means is shown in FIG.
As shown in the figure, the piezoelectric element 23 is installed on the back surface of the sample piece probe holder 8, and the ultrasonic vibration of the resonance state of the sample piece probe holder 8 is given by the piezoelectric element 23, and the sample piece probe 7
The contact can be detected by measuring the disturbance of the resonance state due to the contact of the tip of the sensor.
【００２９】また、図８（b）に示すように、接触によ
って発生する試料片プローブホルダ8の弾性変形を、試
料片プローブホルダ8の裏面に歪みゲージ25を貼付け抵
抗変化を測定することによって接触検知を行なうことで
ある。As shown in FIG. 8B, the elastic deformation of the sample probe holder 8 caused by the contact is measured by attaching a strain gauge 25 to the back surface of the sample probe holder 8 and measuring the resistance change. It is to perform detection.
【００３０】さらに図８で、本発明による第１、第２の
試料作成装置における試料片プローブホルダ8が試料片
プローブ7を保持する手段として、試料片プローブホル
ダ8の表面に窒化アルミ等を絶縁膜としジョンソンラー
ベック力による吸着力を発生する双極型の静電チャック
24を形成する。Further, referring to FIG. 8, the sample piece probe holder 8 in the first and second sample preparation apparatuses according to the present invention is used as a means for holding the sample piece probe 7 by insulating aluminum nitride or the like on the surface of the sample piece probe holder 8. A bipolar electrostatic chuck that generates a chucking force by Johnson-Rahbek force as a film
Form 24.
【００３１】さて、上記の第１、第２の試料作成装置の
観察用試料ホルダ10と観察用試料ホルダ16の取り扱い方
法であるが、処理毎に観察用試料ホルダは交換しなけれ
ばならないが、これを試料処理室1を毎回大気状態にし
て交換することは時間的に効率的ではない。これを改善
するために、観察用試料ホルダ移動機構にエアーロック
構造を備えることによって、観察用試料ホルダを挿入お
よび抜き取りの際に試料処理室を大気にさらさないこと
が必要である。Now, the method of handling the observation sample holder 10 and the observation sample holder 16 of the first and second sample preparation apparatuses described above. The observation sample holder must be replaced for each processing. It is not efficient in terms of time to replace the sample processing chamber 1 with the atmosphere every time. In order to improve this, it is necessary to prevent the sample processing chamber from being exposed to the atmosphere when inserting and extracting the observation sample holder by providing the observation sample holder moving mechanism with an air lock structure.
【００３２】以下、手段そのものは公知であるが、観察
用試料ホルダのエアーロックをいかにして行なうかを図
６で説明する。このエアーロック構造は前方軸シール2
1、後方軸シール20と遮断弁19および前方軸シール21、
後方軸シール20の間の空間を真空排気する手段として真
空ポンプ22を備えることによって構成される。ここで、
例えば、観察用試料ホルダ16を挿入する場合、前方軸シ
ール21を観察用試料ホルダ16が通過する段階では、遮断
弁19は後方軸シール20に当たった状態で閉じている。Hereinafter, how to air-lock the sample holder for observation will be described with reference to FIG. This air lock structure is a front shaft seal 2
1, rear shaft seal 20, shut-off valve 19 and front shaft seal 21,
The vacuum pump 22 is provided as a means for evacuating the space between the rear shaft seals 20. here,
For example, when the observation sample holder 16 is inserted, at a stage where the observation sample holder 16 passes through the front shaft seal 21, the shut-off valve 19 is closed while being in contact with the rear shaft seal 20.
【００３３】また、前方軸シール21、後方軸シール20の
間の空間は真空排気されているため、試料処理室1は真
空状態を保持できている。次に、後方軸シール20を観察
用試料ホルダ16が通過する段階では、すでに、前方軸シ
ール21によって観察用試料ホルダ16の通過部分は真空状
態であるため、遮断弁19を開放しても、試料処理室1は
真空状態を保持できている。逆に、観察用試料ホルダ16
を抜き取る際も同様な真空保持ができるため試料処理室
1を大気にさらすことはない。Since the space between the front shaft seal 21 and the rear shaft seal 20 is evacuated, the sample processing chamber 1 can maintain a vacuum state. Next, at the stage where the observation sample holder 16 passes through the rear shaft seal 20, since the passage portion of the observation sample holder 16 is already in a vacuum state by the front shaft seal 21, even if the shutoff valve 19 is opened, The sample processing chamber 1 can maintain a vacuum state. Conversely, the observation sample holder 16
The same vacuum can be maintained when extracting the sample, so the sample processing chamber
Never expose 1 to the atmosphere.
【００３４】[0034]
【発明の効果】本発明によると、微少な試料片の一連の
ハンドリングに人手をほとんど介さず、しかも、試料処
理室内の真空環境での一貫した試料作成処理が可能とな
り、従来の方式に対し、時間およびコストを削減できる
ばかりか、観察試料面の汚染やダメージの可能性を無く
すことができる。According to the present invention, a series of small sample pieces can be handled with little manual operation, and a consistent sample preparation process can be performed in a vacuum environment in the sample processing chamber. Not only time and cost can be reduced, but also the possibility of contamination and damage of the observation sample surface can be eliminated.
【図１】本発明による第１の試料作成装置の基本構成を
示す概略図。FIG. 1 is a schematic diagram showing a basic configuration of a first sample preparation device according to the present invention.
【図２】本発明による第１の試料作成装置の基本構成を
示す要部概略図。FIG. 2 is a main part schematic diagram showing a basic configuration of a first sample preparation apparatus according to the present invention.
【図３】本発明による第１の試料作成方法を示す説明
図。FIG. 3 is an explanatory view showing a first sample preparation method according to the present invention.
【図４】本発明による第１の試料作成方法を示す説明
図。FIG. 4 is an explanatory view showing a first sample preparation method according to the present invention.
【図５】本発明による第１の試料作成方法を示す斜視
図。FIG. 5 is a perspective view showing a first sample preparation method according to the present invention.
【図６】本発明による第２の試料作成装置の基本構成を
示す概略図。FIG. 6 is a schematic diagram showing a basic configuration of a second sample preparation device according to the present invention.
【図７】本発明による第２の試料作成方法を示す斜視
図。FIG. 7 is a perspective view showing a second sample preparation method according to the present invention.
【図８】本発明による試料片プローブの先端の接触検知
の手段を示した側面図。FIG. 8 is a side view showing a means for detecting contact of the tip of the sample piece probe according to the present invention.
【図９】従来の技術の説明図。FIG. 9 is an explanatory diagram of a conventional technique.
1…試料処理室、2…集束イオンビーム照射光学系、3…
二次電子検出器、4…デポジション用ガス源4、5…元試
料、6…試料移動機構、7…試料片プローブ、8…試料片
プローブホルダ、9…試料片プローブ移動機構、10…観
察用試料ホルダ、11…観察用試料ホルダ移動機構、12…
チャックプレート、13…傾斜スペーサ、14…カンチレバ
ー、15…試料片、16…観察用試料ホルダ、17…元試料、
18…観察用試料ホルダ移動機構、19…遮断弁、20…後方
軸シール、21…前方軸シール、22…真空ポンプ、23…圧
電素子、24…静電チャック、25…歪みゲージ、101…ウ
エハ、102…短冊状ペレット、103…半円形金属板、104
…TEM観察用ホルダ。1… Sample processing chamber, 2… Focused ion beam irradiation optical system, 3…
Secondary electron detector, 4… Deposition gas source 4, 5… Original sample, 6… Sample moving mechanism, 7… Sample piece probe, 8… Sample piece probe holder, 9… Sample piece probe moving mechanism, 10… Observation Sample holder for observation, 11… Sample holder moving mechanism for observation, 12…
Chuck plate, 13: inclined spacer, 14: cantilever, 15: specimen, 16: specimen holder for observation, 17: original specimen,
18: observation sample holder moving mechanism, 19: shut-off valve, 20: rear shaft seal, 21: front shaft seal, 22: vacuum pump, 23: piezoelectric element, 24: electrostatic chuck, 25: strain gauge, 101: wafer , 102: rectangular pellet, 103: semicircular metal plate, 104
... TEM observation holder.
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｇ０１Ｎ 1/28 Ｗ (72)発明者 富松 聡 東京都国分寺市東恋ケ窪一丁目280番地 株式会社日立製作所中央研究所内 (72)発明者 松島 勝 東京都国分寺市東恋ケ窪一丁目280番地 株式会社日立製作所中央研究所内Continued on the front page (51) Int.Cl. 7 Identification FI FI Theme Court II (Reference) G01N 1/28 W (72) Inventor Satoshi Tomimatsu 1-280 Higashi-Koikekubo, Kokubunji-shi, Tokyo Inside Central Research Laboratory, Hitachi, Ltd. (72 Inventor Masaru Matsushima 1-280 Higashi Koigakubo, Kokubunji-shi, Tokyo Inside the Central Research Laboratory, Hitachi, Ltd.
Claims (8)
による観察対象となる試料片を、元試料から成形、分離
および試料片プローブによる採取までの一連のサンプリ
ング工程と、成形後の前記試料片が接続された前記試料
片プローブを観察用試料ホルダに設置するまでの移載工
程を、集束イオンビーム照射光学系および二次電子検出
器と、集束イオンビームの照射領域にデポジション膜を
形成するためのデポジション用ガス源と、元試料を設置
する試料移動機構と、前記試料片を採取するための試料
片プローブと、前記試料片プローブが着脱可能な試料片
プローブホルダおよび試料片プローブ移動機構と、前記
試料片プローブ単体を搭載する観察用試料ホルダおよび
観察用試料ホルダ移動機構を試料処理室に備えることに
よって、前記試料処理室内で一貫して行うことを特徴と
する試料作成装置。1. A series of sampling steps from forming an original sample to a sample to be observed by a transmission electron microscope or a scanning electron microscope to forming, separating, and collecting by a sample piece probe, The transfer process until the connected sample strip probe is set on the observation sample holder is performed by using a focused ion beam irradiation optical system and a secondary electron detector, and forming a deposition film in an irradiation region of the focused ion beam. A deposition gas source, a sample moving mechanism for installing an original sample, a sample piece probe for collecting the sample piece, a sample piece probe holder and a sample piece probe moving mechanism to which the sample piece probe is detachable. By providing an observation sample holder for mounting the sample piece probe alone and an observation sample holder moving mechanism in a sample processing chamber, Sample preparation device and performs consistently in physical room.
前記元試料を前記試料片プローブとともに前記観察用試
料ホルダに設置したことを特徴とする試料作成装置。2. The sample preparation apparatus according to claim 1, wherein
A sample preparation apparatus, wherein the original sample is placed on the observation sample holder together with the sample piece probe.
装置による試料作成方法であって、前記元試料の表面に
試料片として採取する位置を判別する目印を付けるマー
キング工程と、前記観察用試料ホルダにあらかじめ載せ
られている前記試料片プローブを、前記試料片プローブ
ホルダに持ち替える試料片プローブ持ち替え工程と、前
記試料移動機構もしくは前記観察用試料ホルダに設置さ
れている前記元試料に対し、集束イオンビーム照射によ
る前記目印の周辺に複数の垂直矩形穴の加工と、前記試
料移動機構もしくは前記観察用試料ホルダを傾斜させて
行なう斜め矩形穴の加工の組み合わせによって、前記元
試料と片持ち状態でつながっているクサビ形状の試料片
に成形する試料片成形工程と、前記試料片プローブの先
端を前記試料片表面の所定位置に移動し接触させる試料
片プローブ接触工程と、デポジション用ガスを照射しつ
つ前記試料片プローブ先端と前記試料片表面の接触部分
に集束イオンビームを照射してデポジション膜を形成す
ることによって前記試料片プローブと前記試料片を接続
する試料片接続工程と、集束イオンビームを照射するこ
とによって前記元試料と前記試料片とが片持ち状態でつ
ながっている部分を除去する試料片分離工程と、前記試
料片プローブを前記観察用試料ホルダに移載する試料片
プローブ移載工程を順次行なうことを特徴とする試料作
成方法。3. A sample preparation method using the sample preparation apparatus according to claim 1 or 2, wherein a marking step is provided on a surface of the original sample to determine a position at which a sample piece is to be collected, and the observation is performed. The sample piece probe previously mounted on the sample sample holder, the sample piece probe replacement step of holding the sample piece probe holder, and for the original sample placed in the sample moving mechanism or the observation sample holder, The original sample is cantilevered by a combination of processing of a plurality of vertical rectangular holes around the mark by focused ion beam irradiation and processing of the oblique rectangular holes performed by tilting the sample moving mechanism or the observation sample holder. A sample piece forming step of forming a wedge-shaped sample piece connected by A sample piece probe contacting step of moving to a predetermined position and making contact therewith, and irradiating a focused ion beam to a contact portion between the tip of the sample piece probe and the surface of the sample piece while irradiating a deposition gas to form a deposition film. A sample piece connecting step of connecting the sample piece probe and the sample piece, and a sample piece separation step of irradiating a focused ion beam to remove a portion where the original sample and the sample piece are connected in a cantilever state. And a sample probe transfer step of transferring the sample strip probe to the observation sample holder.
前記試料片分離工程と試料片プローブ移載工程の間に、
前記試料片に対して、前記目印をもとに透過型電子顕微
鏡による観察のための薄壁部を形成する薄壁部形成工程
を含むことを特徴とする試料作成方法。4. The sample preparation method according to claim 3, wherein
Between the sample piece separation step and the sample piece probe transfer step,
A method for forming a sample, comprising: forming a thin wall portion on the sample piece for observation by a transmission electron microscope based on the mark.
片プローブ接触工程において、前記試料片プローブの先
端が前記元試料の表面に接触したことを検知する手段と
して、前記試料片プローブホルダに圧電素子によって共
振状態の超音波振動を与え、前記試料片プローブの接触
による共振状態の乱れを測定することによって上記接触
検知を行なうことを特徴とする試料作成装置。5. The sample piece probe holder according to claim 3, wherein in the sample piece probe contacting step, the sample piece probe holder is used as means for detecting that the tip of the sample piece probe has contacted the surface of the original sample. A sample preparation apparatus for applying ultrasonic vibration in a resonance state to the sample piece probe and measuring disturbance of the resonance state caused by contact of the sample piece probe.
片プローブ接触工程において、前記試料片プローブの先
端が前記試料片プローブの表面に接触したことを検知す
る手段として、接触によって発生する前記試料片プロー
ブホルダの弾性変形を、前記試料片プローブホルダに歪
みゲージを貼付け、前記歪みゲージの抵抗変化を測定す
ることによって上記接触検知を行なうことを特徴とする
試料作成装置。6. The sample-probe contacting step of the sample preparation method according to claim 3, wherein the contact is generated by contact as a means for detecting that the tip of the sample-probe has contacted the surface of the sample-probe. A sample preparation device, wherein the elastic deformation of the sample piece probe holder is detected by attaching a strain gauge to the sample piece probe holder and measuring a change in resistance of the strain gauge.
装置において、前記試料片プローブホルダが前記試料片
プローブを保持する手段として、静電チャックを用いた
ことを特徴とする試料作成装置。7. The sample preparation apparatus according to claim 1, wherein said sample piece probe holder uses an electrostatic chuck as means for holding said sample piece probe. .
装置において、観察用試料ホルダ移動機構にエアーロッ
ク構造を備え、前記観察用試料ホルダを挿入または抜き
取りの際に前記試料処理室を大気にさらさないことを特
徴とする試料作成装置。8. The sample preparation apparatus according to claim 1, further comprising an air lock structure provided in the observation sample holder moving mechanism, wherein the sample processing chamber is inserted when the observation sample holder is inserted or withdrawn. A sample preparation device characterized by not being exposed to the atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33223798A JP4126786B2 (en) | 1998-11-24 | 1998-11-24 | Sample preparation apparatus and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33223798A JP4126786B2 (en) | 1998-11-24 | 1998-11-24 | Sample preparation apparatus and method |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2008057169A Division JP4483957B2 (en) | 2008-03-07 | 2008-03-07 | Sample preparation device |
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| Publication Number | Publication Date |
|---|---|
| JP2000155081A true JP2000155081A (en) | 2000-06-06 |
| JP2000155081A5 JP2000155081A5 (en) | 2005-12-08 |
| JP4126786B2 JP4126786B2 (en) | 2008-07-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33223798A Expired - Lifetime JP4126786B2 (en) | 1998-11-24 | 1998-11-24 | Sample preparation apparatus and method |
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